CN109153617A

CN109153617A - The Polycrystalline Cubic Boron Nitride of sintering

Info

Publication number: CN109153617A
Application number: CN201780031384.5A
Authority: CN
Inventors: A·M·M·莫特切拉霍; S·高希; A·坎
Original assignee: Element Six UK Ltd
Current assignee: Element Six UK Ltd
Priority date: 2016-06-02
Filing date: 2017-05-31
Publication date: 2019-01-04
Also published as: JP2023002580A; GB201708616D0; EP3464217A1; KR102358312B1; EP3464217B1; GB201609672D0; JP2019521941A; GB2552408B8; GB2552408B; WO2017207601A1; KR20210008147A; JP7384770B2; US20190119167A1; KR20190003696A; US11518717B2; JP2020203834A; US20230079359A1; GB2552408A

Abstract

Polycrystalline cubic boron nitride PCBN material and the method for manufacturing PCBN.Method includes providing the matrix precursor powder of the particle comprising average particle size particle size no more than 250nm, the cubic boron nitride cBN powder for the cBN particle for being at least 0.2 μm comprising average particle size particle size is provided, matrix precursor powder and cBN powder are closely mixed, and be sintered the powder closely mixed at least 1100 DEG C of temperature and the pressure of at least 3.5GPa to form PCBN material, which includes the particle for the cubic boron nitride cBN being dispersed in host material.

Description

The Polycrystalline Cubic Boron Nitride of sintering

Technical field

The present invention relates to sintered polycrystalline cubic boron nitride material fields, and the method for this material of manufacture.

Background technique

Plycrystalline diamond superhard material can be used for various tools such as polycrystalline diamond (PCD) and polycrystalline cubic boron nitride (PCBN), For cut, machine, drill or degrade hard or abrasive material, such as rock, metal, ceramics, composite material and contain timber Material.

Abrasive compacts are widely used in cutting, milling, grind (grinding), drilling and other grindings (abrasive) behaviour Make.They usually contain the superabrasive particles being dispersed in the second phase matrix.Matrix can be metal or ceramics or metal pottery Porcelain.Superabrasive particles can be diamond, cubic boron nitride (cBN), silicon carbide or silicon nitride etc..In usually used high pressure During being compacted manufacturing process with high temperature, these particles can be bonded to each other, to form plycrystalline diamond substance, or can pass through second The matrix of phase material is combined to form the plycrystalline diamond object of sintering.This type objects is commonly known as polycrystalline diamond or polycrystalline cubic nitrogen Change boron, wherein they separately include diamond or cBN as super hard abrasive.

United States Patent (USP) US 4,334,928 teaches a kind of sintered compact for tool, substantially by 20 to 80 bodies The cubic boron nitride composition of product %；And surplus is the matrix of at least one matrix compounds material, the matrix compounds material Carbide, nitride, carbonitride, boride and the silicide of IVa or Va transition metal of the material selected from periodic table, they mixed Close the solid solution compound of object and they.The matrix forms continuous glued construction in sintered body, wherein high pressure boron nitride It is dispersed in continuous matrix.The method summarized in the patent is all referred to using mechanical lapping/hybrid technology (such as ball milling, mortar etc.) To merge material requested.

They can be and being formed in substrate by " support " by the plycrystalline diamond object of sintering.It can be used to form suitable substrates Bonding tungsten carbide be to be formed by the carbide particle being dispersed in such as cobalt matrix, by by tungsten carbide particle/crystal grain and cobalt It mixes and then is heating and curing.In order to form the cutting element with ultra hard material layer (such as PCD or PCBN), in infusibility gold Belong in shell (such as niobium shell), diamond particles or crystal grain or CBN crystal grain are placed on bonding tungsten carbide near vicinity, and It is subjected to high pressure and high temperature makes that intercrystalline bonding occurs between diamond crystals or CBN crystal grain, to form the superhard Buddha's warrior attendant of plycrystalline diamond Stone or CBN layers of plycrystalline diamond.

In some cases, substrate can be fully cured before being attached to ultra hard material layer, and in other cases, base Bottom can be green compact state (not being fully cured).In the latter case, substrate can be fully cured during HTHP sintering process.Base Bottom can be powder type, and can solidify during the sintering process for being sintered ultra hard material layer.

Fig. 1 shows the illustrative methods for manufacturing sintering PCBN material.Number corresponds to the number of Fig. 1 below:

S1. matrix precursor powder is pre-mixed.The example of matrix precursor powder includes carbide and/or the nitridation of titanium and aluminium Object.The exemplary average grain size of matrix precursor powder is 1 to 10 μm.

S2. matrix precursor powder is heat-treated at more than 1000 DEG C at least one hour, with cause matrix precursor granules it Between pre-reaction to forming " pie " (cake).

S3. pie is crushed and is sieved to obtain the particle of required grade.

S4. before cubic boron nitride (cBN) particle that average particle size particle size is 0.5 to 15 μm being added to the matrix after sieving In body powder.

S5. gained mixed-powder is milled so that matrix precursor powder is crushed to desired size (being typically 50 to 700nm) And mix matrix precursor powder closely with cBN particle.The process may need a few hours, and be related to using such as tungsten carbide The abrasive media of ball.

S6. obtained abrasive flour is dry to remove solvent at 60 DEG C or more under vacuum or low pressure, then by slow Slowly make oxygen enter system to be adjusted with passivating metallic surfaces (such as aluminium).

S7. dry powder is sieved and prepares pre-composite sub-assembly.

S8. pre-composite sub-assembly is heat-treated at 700 DEG C or more, to remove the water or gas of any absorption.

S9. the pre-composite sub-assembly of degassing is assembled into the involucrum for being suitable for sintering.

S10. involucrum is sintered at least 1250 DEG C and at least 4GPa high pressure-temperature (HPHT) technique to form sintering PCBN material.

Entire technique is very time-consuming and may need up to five days on a commercial scale.

During (attrition mill) process of milling, powder can be from abrasive media suck up impurity.Fig. 2 is sintering PCBN The microphoto of material, wherein being milled with tungsten-carbide ball.White particle (example is highlighted with black circles) is carbon Change tungsten particle.The PCBN material of sintering contains the at most tungsten carbide of 8 weight %.Property of these the known particles to PCBN material It has adverse effect, especially in the application of such as hard part turning.In addition, the tungsten carbide drawn during mill not by Control, therefore different batches may include different amounts of tungsten carbide, have different sizes distribution, so as to cause work is being used for Sintering PCBN material has uncertain performance when tool application.

Summary of the invention

Purpose is to provide a kind of sintering PCBN material, has the tungsten carbide content being greatly reduced.

According in a first aspect, providing a kind of method for manufacturing PCBN material.Offer is not more than comprising average particle size particle size The matrix precursor powder of the particle of 250nm.The cBN powder for the cBN particle for being at least 0.2 μm comprising average particle size particle size is also provided End.Matrix precursor powder and cBN powder are closely mixed.Temperature and at least by the powder closely mixed at least 1100 DEG C To form PCBN material, which includes the cubic boron nitride being dispersed in host material for sintering under the pressure of 3.5GPa The particle of cBN.One advantage of this method is not use abrasive media, therefore obtained PCBN is free of from the miscellaneous of abrasive media Matter, such as tungsten carbide.Another advantage is not need step of milling, therefore the total time for preparing PCBN is reduced.Another advantage It is that the small size of matrix precursor particle keeps them bigger in sintering step present invention.

As a kind of selection, this method includes before providing the matrix comprising particle of the average particle size particle size no more than 100nm Body powder.

The step of matrix powder and cBN powder are closely mixed optionally includes matrix precursor powder and cBN powder point It dissipates in a solvent, using ultrasonic mixer mixed solvent, matrix precursor powder and cBN powder, and removes solvent to leave The powder of matrix precursor particle and cBN particle closely mixed.

As a kind of alternative, the step of matrix powder and cBN powder are closely mixed includes dry type acoustic mixing.

As a kind of selection, this method includes the cBN powder particle for providing average-size between 0.2 and 15 μm.CBN Grain optionally has the average-size greater than 1 μm.As a further alternative, the average-size of cBN particle is at 5 μm to 10 μm In range.

CBN particle optionally has multi-modal average-size distribution.

Obtained PCBN material optionally includes less than the cBN particle of 80 volume %.

As a kind of selection, host material includes the material of compound any in titanium and aluminium.Exemplary substrates material Material includes any in titanium carbonitride, titanium carbide, titanium nitride, titanium diboride, aluminium nitride and aluminium oxide.

According to second aspect, a kind of method for manufacturing PCBN material is provided.This method includes providing the base comprising particle Matter precursor powder.Matrix precursor powder is milled using abrasive media to realize the average particle size particle size for being not more than 1 μm.By grinding Matrix precursor powder is closely mixed with the cBN powder for the particle for being at least 0.2 μm comprising average particle size particle size.By what is closely mixed Powder is sintered to form PCBN material at least 1100 DEG C of temperature and the pressure of at least 3.5GPa, which includes point It is dispersed in the particle of the cubic boron nitride cBN in host material.One advantage of this method is that gained PCBN material has less than 0.5 The low-down impurity content from abrasive media of weight %, because without milling after cBN is added.

As a kind of selection, the step of matrix powder and cBN powder are closely mixed includes by ground matrix precursor Powder and the dispersion of cBN powder in a solvent, using ultrasonic mixer mixed solvent, matrix precursor powder and cBN powder, and remove Solvent is removed to leave the powder of matrix precursor particle and cBN particle closely mixed.Alternatively, by surface-active Agent is added in solvent.

As a kind of selection, ground matrix precursor powder includes the particle that average particle size particle size is not more than 200nm.

CBN particle optionally has 0.2 to 15 μm, or the average-size greater than 1 μm.CBN particle optionally has multimode The distribution of state average-size.

As a kind of selection, host material includes the material of compound any in titanium and aluminium.Exemplary materials packet It includes any in titanium carbonitride, titanium carbide, titanium nitride, titanium diboride, aluminium nitride and aluminium oxide.

As a kind of selection, matrix precursor powder is milled to realize the average particle size particle size for being not more than 700nm.As another A kind of selection mills matrix precursor powder to realize the average particle size particle size for being not more than 500nm.

According to the third aspect, a kind of polycrystalline cubic boron nitride (PCBN) material is provided.The PCBN material includes to be dispersed in The particle of cubic boron nitride (cBN) in host material, the host material include at least one titanium-containing compound.The PCBN material The impurity from abrasive media comprising being not more than 0.5 weight %.

As a kind of selection, PCBN material does not include abrasive media impurity.

Abrasive media impurity is optionally included selected from tungsten carbide, silicon carbide, aluminium oxide, zirconium oxide, titanium carbide and boron carbide In any material because they are typically used as the abrasive media milled.

CBN particle optionally has 0.2 to 15 μm of average-size.As a further alternative, cBN particle has and is greater than 1 μm of average-size.

As a kind of selection, there is cBN particle multi-modal average-size to be distributed.

PCBN material optionally includes less than the cBN particle of 80 volume %.

Host material optionally includes the material of any compound in titanium and aluminium.Alternatively, matrix Material includes any in titanium carbonitride, titanium carbide, titanium nitride, titanium diboride, aluminium nitride and aluminium oxide.

According to fourth aspect, a kind of tool is provided comprising the sintered polycrystalline material as described in the third aspect, the work Tool for cutting, milling, grind, drill or it is other grinding application in it is any.

Brief description

Example will be passed through now and non-limiting embodiments are described in reference to the drawings, in which:

Fig. 1 is the flow chart for showing the known example method of manufacture sintering PCBN material；

Fig. 2 is the microphoto for showing the exemplary sintering PCBN material of the manufacture of the step according to Fig. 1；

Fig. 3 is to show that manufacture there is no the stream of the illustrative steps of the method for the sintering PCBN material of tungsten carbide content Cheng Tu.

Fig. 4 is to show that manufacture has the illustrative steps of the method for the sintering PCBN material for the tungsten carbide content being greatly reduced Flow chart；

Fig. 5 is the flow chart for showing the illustrative steps of method of sintering PCBN material of the manufacture without tungsten carbide.

Fig. 6 is to show that manufacture has the illustrative steps of the method for the sintering PCBN material for the tungsten carbide content being greatly reduced Flow chart；

Fig. 7 is the scanning electron micrograph without the sample of tungsten carbide manufacture；

Fig. 8 is the scanning electron micrograph of the sample manufactured with extremely low tungsten carbide；

The X-ray diffractogram of Fig. 9 shows the presence of the tungsten carbide of the prior art PCBN material using manufacture of milling；

The X-ray diffractogram of Figure 10 shows the only exemplary PCBN material to adhesive precursor powder using manufacture of milling Tungsten carbide presence；

Figure 11 shows that the flank of the actual measurement of the tool manufactured in H05 machining test using PCBN material is wear-resisting Property；With

Figure 12 shows that the crescent hollow abrasion of the actual measurement of the tool manufactured in H05 machining test using PCBN material is resistance to By property.

It is described in detail

Inventors have realised that can be eliminated during step of milling by eliminating step of milling from abrasive media Impurity presence.It mills and is applied not only to matrix precursor Particle Breakage into required size, but also be used for matrix precursor Particle and cBN particle closely mix and disperse.In the first embodiment, it has been found that use size needed for having had suitably Matrix precursor powder, and come close mixed-matrix precursor granules and cBN particle using the technology except milling and can result in Sintering PCBN material without abrasive media impurity.

Fig. 3 is turned to, the flow chart for showing the illustrative steps according to first embodiment is shown.Number corresponds to below The number of Fig. 3:

S11. the nano particle of matrix precursor powder is provided, which has the average particle size particle size no more than 200nm.

S12., cBN powder is also provided.The average-size of cBN particle in cBN powder is at least 0.2 μm.The size of cBN point Cloth can be single mode or multi-modal (including bimodal).

S13. it is used without the technology of abrasive media, such as is mixed by ultrasonic mixing in a solvent or by dry type acoustics It closes, cBN powder and matrix precursor powder is closely mixed.

S14. the temperature and at least 3.5GPa by mixed-powder in high pressure-temperature (HPHT) press at least 1100 DEG C It is sintered under pressure, to form the PCBN material for including cBN particle in the matrix containing at least one titanium compound.It is exemplary Host material be titanium carbonitride, titanium carbide, titanium nitride, titanium diboride, aluminium nitride and aluminium oxide.There may also be other materials Material, such as the compound based on hafnium.

Obtained sintering PCBN material does not contain tungsten carbide, or the other impurity usually generated by abrasive media, because There is no the steps of milling using tungsten carbide.Other than preparing the PCBN without tungsten carbide or other abrasive media impurity, lack Milling less means that the time of preparation sintering PCBN material is greatly decreased with pre-reaction step.Nano particle is used for precursor matrix The advantages of powder is that they have the high surface area therefore quite reactive during sintering.

Although nanometer powder is used to matrix precursor powder to have many advantages, the matrix precursor powder of nano-scale is used End may be not always suitable.It can lead to powder handling issues comprising short grained nanometer powder, such as agglomeration and reply are received The intensified response at rice flour end.Inventors have realised that most of absorption objects from abrasive media during milling It (pickup) is as caused by the presence of cBN.The abrasive media of such as tungsten-carbide ball is harder than matrix precursor powder, therefore matrix Precursor powder is less likely degradation tungsten-carbide ball.However, cBN is harder than tungsten-carbide ball, therefore can make tungsten-carbide ball degrade, thus Tungsten carbide is caused to be drawn.

In second specific embodiment, matrix precursor powder is milled to reduce matrix in the case where cBN is not present The particle size of precursor powder.Then cBN particle is added in matrix precursor powder and is closely mixed, then compacting and sintering To form the PCBN material of sintering.It has been found that the technology can lead to the PCBN material of sintering, which, which has, is less than The tungsten carbide of 0.5% weight percent.

Fig. 4 is turned to, is the flow chart for showing the illustrative steps according to the second embodiment.Number corresponds to figure below 4 number:

S15., matrix precursor powder is provided.

S16. it is milled using abrasive media such as tungsten-carbide ball to matrix precursor powder, to reduce particle size and close Mixed-matrix precursor powder.Average particle size particle size is reduced at most 700nm.Typically, this can be about 200 to 250nm.

S17. after milling, before removing abrasive media and cBN particle being added to ground matrix with required amount In body powder.

S18. it is used without the technology of abrasive media, such as by ultrasonic mixing in a solvent or passes through dry type acoustics Mixing, mixed-matrix precursor powder and cBN particle are closely mixed.

S19. the temperature and at least 3.5GPa by mixed-powder in high pressure-temperature (HPHT) press at least 1100 DEG C It is sintered under pressure, to form the PCBN material for including cBN particle in the matrix containing at least one titanium compound.Illustratively Host material is titanium carbonitride, titanium carbide, titanium nitride, titanium diboride, aluminium nitride and aluminium oxide.There may also be other materials, Such as the compound based on hafnium.

The powder-processed that technology described in Fig. 4 encounters when overcoming in the first embodiment using nanometer powder Some problems.There are the absorptions of a small amount of tungsten carbide during the milling of matrix precursor powder, but sight when being milled with cBN particle The tungsten carbide uptake observed is compared, this is negligible.There is the PCBN material of sintering the tungsten carbide less than 0.5 weight % to contain Amount.

For both above-mentioned first and second embodiments, exists and closely mix matrix precursor powder with cBN particle Step.As described above, this can be completed by ultrasonic mixing.This can be dispersed the powder into this case in a solvent In solvent, then ultrasonic mixing removes solvent.Surfactant can be added with the powder in solvent stability.Exemplary solvent packet Include hexane, ethyl alcohol and isopropanol.

Embodiment

As shown in Figure 3, first group of embodiment PCBN material is manufactured using the matrix precursor powder comprising nanometer powder.Figure 5 illustrate in greater detail step, and number corresponds to the number of Fig. 5 below:

S20. the average particle size particle size of nanomatrix precursor powder is about 50nm to 100nm.Prepare various host materials.

S21. matrix precursor powder is closely mixed using ultrasonic mixer in various solvents.Ultrasonic mixer is Branson 2000bdc, 20kHz, 2.2kW all-wave, 50mm diameter loudspeaker, amplitude 40-60%.

S22. cubic boron nitride (cBN) particle is added in mixed-matrix precursor powder.

S23. by mixed-matrix precursor powder and cBN particle ultrasonic mixing 20 minutes.

S24. by obtained mixed-powder in low pressure (less than 500 millibars) and 60 DEG C or more dryings to remove solvent.Pass through It introduces oxygen slowly to provide the passivation of any aluminium surface, (condition) is adjusted to powder.

S25. dry powder is sieved and prepares pre-composite sub-assembly.

S26. pre-composite sub-assembly is heat-treated 2 hours in the case where being greater than 1025 DEG C, to remove the water or gas of any absorption. The heat treatment can be carried out under low pressure.

S27. the pre-composite sub-assembly of degassing is assembled into the involucrum for being suitable for sintering.

S28. involucrum is sintered under 1250 DEG C and 5.5GPa in HPHT press to form sintering PCBN material.

Reference PCBN material also is prepared using technology shown in FIG. 1, to show that the material of abrasive media is milled and drawn to experience Material, and have no chance to draw the difference between the PCBN material of any abrasive media.

Table 1 shows the composition and some Fabrication parameters of embodiment.

Table 1

As shown in figure 4, manufacturing second of PCBN material by milling matrix precursor powder before adding cBN.Fig. 6 is more Step is shown in detail, number corresponds to the number of Fig. 6 below:

S29. matrix precursor powder of the premixing with 1 to 10 μm of average particle size particle size.

S30. matrix precursor powder is heat-treated at least 1 hour at about 1025 DEG C, to cause between matrix precursor granules Pre-reaction and formation " pie ".

S31. pie is crushed and is sieved to obtain the particle of required grade.

S32.Gained powder is milled so that matrix precursor powder is crushed to desired size (being typically 50 to 700nm) and is made Matrix precursor powder closely mixes.It is milled using tungsten carbide milling media.

S33. cubic boron nitride (cBN) particle is added in mixed-matrix precursor powder.

S34. by mixed matrix powder and cBN particle ultrasonic mixing 20 minutes.

S35. by obtained mixed-powder in low pressure (less than 500 millibars) and 60 DEG C or more dryings to remove solvent.Pass through It introduces oxygen slowly to provide the passivation of any aluminium surface, powder is adjusted.

S36. dry powder is sieved and prepares pre-composite sub-assembly.

S37. pre-composite sub-assembly is heat-treated 2 hours in the case where being greater than 1025 DEG C, to remove the water or gas of any absorption. The heat treatment can be carried out under low pressure.

S38. the pre-composite sub-assembly of degassing is assembled into the involucrum for being suitable for sintering.

S39. involucrum is sintered under 1250 DEG C and 5.5GPa in HPHT press to form sintering PCBN material.

Table 2 shows the composition and some Fabrication parameters of the embodiment according to Fig. 6 manufacture.

Table 2

Embodiment	CBN volume %	Matrix forms weight %	Solvent
				18	60	45TiC/45TiN/10Al	Hexane

Fig. 7 is the scanning electron micrograph of embodiment 9.It is different from Fig. 2, not there is tungsten carbide because not into Capable step of milling.Fig. 8 is the scanning electron micrograph of embodiment 18.In this case, there are very small amount of tungsten carbides.Carbon The example for changing tungsten particle is highlighted with white circle.The amount of tungsten carbide is about 0.2 weight % according to estimates.

Tungsten carbide trace is not shown in the X-ray diffraction (XRD) of embodiment 1 to 17.In contrast, the XRD of reference sample The peak for being attributed to tungsten carbide is clearly shown, as shown in Figure 9.In contrast, the XRD trace obtained by embodiment 18 is shown very Small tungsten carbide trace, as is expected.

Some samples are analyzed to measure their density, the velocity of sound (SOS), specific surface area (SSA) and hardness.The data obtained is such as Shown in table 3.

Table 3

Embodiment	Density g/cm³	SOS km/s	SSA g/m²	Vickers hardness GPa
					1	4.21	11.51	22.33	23.79
2	4.22	11.66	22.33	25.33
					3	4.11	11.76	21.14	25.12
4	4.20	11.83	21.14	26.38
					5	4.01	12.60	22.66	27.84
6	4.22	11.45	23.87	26.02
					7	4.19	11.55	23.15	25.56
8	4.20	11.45	25.66	25.38
					9	4.05	12.35	24.44	28.35
Reference	-	12.39	17.11	29-30

Some embodiment PCBN materials are formed into machinery tools and test (V in H05 machining test_c=200m/ Min, feed speed 0.1mm/rev, cutting depth 0.15mm, workpiece SAE8620, hardness 60-62HRC, in a: It is carried out on Glidemeister CTX500 lathe.Use V_BMeasure flank wearability.Embodiment 1,2 and 4 and reference sample Flank wearability it is as shown in figure 11.Sample 1,2 and 4 has the flank wearability slightly improved.

Pass through K_TIt measures crescent hollow abrasion tolerance (also referred to as chemical wear resistance).Compared with reference sample, embodiment 1,2 and 4 all have the crescent hollow abrasion tolerance slightly improved, as shown in figure 12.This improvement is considered as from lower cBN The combination of content and lower tungsten carbide content.

Above-mentioned two specific embodiment respectively provides the mode of production PCBN material, draws without abrasive media Or draw with the abrasive media that substantially reduces (so that abrasive media account for PCBN material less than 0.5 weight %).This allows PCBN material has more controllable and predictable property to be prepared.In addition, the technology also reduce prepare PCBN material when Between.

Another group of exemplary powders are prepared using dry type acoustic mixing technology.In 100ml polyamide tank, by titanium carbonitride (TiC_0.5N_0.5) powder (1.3 μm of average particle size particle sizes) and aluminium (6 μm of average particle size particle sizes) it is pre- with the ratio of 90:10 (weight %) Mixing.36g TiC is weighed in tank_0.5N_0.5With 4g Al, be sealed against being placed in LABRAM I dry type acoustic mixing device and It is run 2 minutes under 40G and in different experiments with 60G operation 2 minutes.

Then by the powder of premixing in conjunction with the cubic boron nitride powder that particle size is 4-5 μm and 6-7 μm, with preparation The compound of 60 volume % and 70 volume %.The second step is combined and is also carried out under the different condition of 40G and 60G.Condition is as follows Shown in table 4.

Table 4

Premixing	After mix	CBN particle size (μm)
			40G,2min	40G,5min	4-5
40G,2min	40G,5min	6-7
			60G,2min	60G,5min	4-5
60G,2min	60G,5min	6-7

Final powder is sintered at about 5.5GPa and 1400 DEG C in belt-type high pressure high-temperature service.Agglomerated material is cut And polish, the microstructure analysis in SEM shows that the microstructure of resulting materials is uniform.

In another set of experiments, individual TiC and TiN powder (1-2 microns of average particle size particle size) are premixed together with 80G It closes 2 minutes.Then 4-5 μm of cBN particle is mixed 30 seconds with TiC/TiN powder with 80G and is mixed 2 minutes with 100G.Another In one step, 6 μm of aluminium are added in system and is mixed 30 seconds with 80G and is mixed 2 minutes with 100G.By powder with enough Amount is mixed to prepare the composition of 60 volume %cBN, and remaining TiC/TiN:Al weight ratio is 90:10.Gained powder and sintering Material analysis shows that be uniform structure.

Finally, 1.3 μm of cBN of 90g are mixed 5 minutes with 6 μm of aluminium of 10g with 80G.Gained microstructure is shown greatly Agglomerate.In another experiment, this is mixed with the amount of 20g in the polyamide tank of 100ml in LABRAM I mixer A little powder, with the 0.7mm WC ball of 200 weight % in tank.It runs mixture 30 seconds with 80G and runs 2 points with 100G Clock.The microstructure of final agglomerated material shows uniform structure.

Definition

As used herein, PCBN material refers to a kind of superhard material, and it includes be dispersed in the matrix including metal or ceramics Interior cBN grains.PCBN is an example of superhard material.

As used herein, " PCBN structure " includes the object of PCBN material.

" host material " is understood to mean that the hole filled in synneusis texture completely or partially, gap or gap area Host material.Term " matrix precursor powder " is for referring to the powder for becoming host material when being subjected to high pressure-temperature sintering process.

The multi-modal size distribution of great number of grains is understood to mean that there is crystal grain the size at more than one peak to be distributed, each Peak corresponds to respective " mode ".Multi-modal plycrystalline diamond object can be manufactured by providing multiple crystal grain in more than one source, often A source includes the crystal grain with dramatically different average-size, and by from these sources crystal grain or particle it is blended together.One In a embodiment, PCBN material may include the cBN grains with multimodal distribution.

Above description is related to average particle size particle size.This is measured using equivalent diameter (ECD) technology.It can be by swashing Optical diffraction measures the ECD distribution of multiple loose, unrestricted and non-agglomeration crystal grain, wherein being randomly provided crystal grain in incident light Path in, and measure light diffraction pattern caused by crystal grain diffraction.Diffraction pattern can mathematically be construed to seem it It is to be generated by multiple spherical particles, diameter distribution is calculated and reported according to ECD.The aspect of grain size distribution can be with It is indicated using various terms and symbol by various statistical properties.The specific example of these terms includes average, intermediate and mode.Ruler Very little distribution may be considered that a series of class value Di for corresponding to corresponding size channels, wherein each Di corresponds to each lead to The geometric average ECD value of road i, i are the integers in the range of 1 to port number n used.

By laser diffraction method obtain average value can the distribution based on crystal particle volume most easily express, according to public affairs The mathematical formulae known, bulk averaged value can be expressed as D [4,3].As a result surface area distribution can be converted to, according to well-known Mathematical formulae, average value be D [3,2].Unless otherwise indicated, then the average value of the distribution of size used in the disclosure refers to Average value D [4,3] based on volume.The median D50 of size distribution is the value that multiple crystal grain are divided into two equal groups, one By having the crystal grain of the ECD size higher than the value to form, the other half has the ECD size of the at most value for a group.Size distribution Mode be value corresponding with the highest frequency of crystal grain, can be rendered as distribution (distribution may include more than one part at peak Maximum frequency and referred to as multi-modal).Various other value d (y) can be provided, the size indicated refers to: depositing in distribution It is lower than the size in multiple crystal grain of score y.For example, d (0.9) refers to that 90% crystal grain is lower than the ECD size of the size, d (0.5) refer to that 50% crystal grain is lower than the ECD size of the size, d (0.1) refers to that 10% crystal grain is lower than the ECD ruler of the size It is very little.

Although the present invention is particularly shown and described by reference to embodiment, those skilled in the art will be managed Solution can carry out each in form and details in the case where not departing from the scope of the invention being defined by the appended claims Kind changes.For example, although all embodiments use cBN as superhard phase, but it is to be understood that identical technology can be used for The other types of superhard material being dispersed in host material.

Claims

1. a kind of method for manufacturing polycrystalline cubic boron nitride PCBN material, this method comprises:

The matrix precursor powder of particle comprising average particle size particle size no more than 250nm is provided；

The cubic boron nitride cBN powder for the cBN particle for being at least 0.2 μm comprising average particle size particle size is provided；

The matrix precursor powder and the cBN powder are closely mixed；With

The powder closely mixed is sintered at least 1100 DEG C of temperature and the pressure of at least 3.5GPa to form PCBN material, The PCBN material includes the particle for the cubic boron nitride cBN being dispersed in host material.

2. the method for manufacture polycrystalline cubic boron nitride PCBN material according to claim 1, further includes providing comprising average The matrix precursor powder of particle of the particle size no more than 100nm.

3. the method for manufacture PCBN material according to claim 1 or 2, wherein matrix powder and cBN powder are closely mixed The step of conjunction includes:

In a solvent by matrix precursor powder and the dispersion of cBN powder；

Use ultrasonic mixer mixed solvent, matrix precursor powder and cBN powder；With

Solvent is removed to leave the powder of matrix precursor particle and cBN particle closely mixed.

4. the method for manufacture PCBN material according to claim 1 or 2, wherein matrix precursor powder and cBN powder is tight The step of close mixing includes dry type acoustic mixing.

5. the method for manufacture PCBN material according to claim 1-4, this method includes providing average-size to exist CBN particle between 0.2 and 15 μm.

6. the method for manufacture PCBN material according to claim 1-5, this method includes that offer average-size is big In 1 μm of cBN particle.

7. the method for manufacture PCBN material according to claim 1-6, this method includes providing average-size 5 μm to the cBN particle in 10 μ ms.

8. the method for manufacture PCBN material according to claim 1-7, this method include providing with multi-modal Average-size distribution cBN particle.

9. wherein the PCBN material includes less than 80 according to the method for the described in any item manufacture PCBN materials of claim 7 to 8 The cBN particle of volume %.

10. the method for -9 described in any item manufacture PCBN materials according to claim 1, wherein the host material includes to be selected from titanium With the material of compound any in aluminium.

11. the method for manufacture PCBN material according to claim 10, wherein the host material includes titanium carbonitride, carbon Change any in titanium, titanium nitride, titanium diboride, aluminium nitride and aluminium oxide.

12. a kind of method for manufacturing polycrystalline cubic boron nitride PCBN material, this method comprises:

Matrix precursor powder comprising particle is provided；

The matrix precursor powder mill to realize the average particle size particle size for being not more than 1 μm；

Honed matrix precursor powder is closely mixed with the cBN powder for the particle for being at least 0.2 μm comprising average particle size particle size； With

13. the method for manufacture PCBN material according to claim 12, wherein matrix powder and cBN powder are closely mixed The step of include:

In a solvent by honed matrix precursor powder and the dispersion of cBN powder；

14. it is according to claim 13 manufacture PCBN material method, this method further include surfactant is added it is molten In agent.

15. the method for manufacture PCBN material according to claim 12, wherein matrix powder and cBN powder are closely mixed The step of include dry type acoustic mixing.

16. the method for the described in any item manufacture PCBN materials of 2-15 according to claim 1, wherein honed matrix precursor powder It is not more than the particle of 200nm comprising average particle size particle size.

17. the method for the described in any item manufacture PCBN materials of 2-16 according to claim 1, this method includes providing to have 0.2 To the cBN particle of 15 μm of average-sizes.

18. the method for the described in any item manufacture PCBN materials of 2-17 according to claim 1, this method includes providing to have to be greater than The cBN particle of 1 μm of average-size.

19. the method for the described in any item manufacture PCBN materials of 2-18 according to claim 1, this method includes providing to have multimode The cBN particle of state average-size distribution.

20. the method for the described in any item manufacture PCBN materials of 2-19 according to claim 1, wherein the PCBN material includes small In the cBN particle of 80 volume %.

21. the method for the described in any item manufacture PCBN materials of 2-20 according to claim 1, wherein the host material includes choosing The material of any compound from titanium and aluminium.

22. the method for manufacture PCBN material according to claim 21, wherein the host material includes titanium carbonitride, carbon Change any in titanium, titanium nitride, titanium diboride, aluminium nitride and aluminium oxide.

23. the method for the described in any item manufacture PCBN materials of 2-22 according to claim 1, this method includes by matrix precursor powder It mills to realize the average particle size particle size for being not more than 700nm at end.

24. the method for the described in any item manufacture PCBN materials of 2-22 according to claim 1, this method includes by matrix precursor powder It mills to realize the average particle size particle size for being not more than 500nm at end.

25. a kind of polycrystalline cubic boron nitride PCBN material, the PCBN material include:

The particle of cubic boron nitride cBN；

The cBN particle is dispersed in host material, and the host material includes at least one titanium-containing compound；

Wherein the PCBN material includes the impurity from abrasive media no more than 0.5 weight %.

26. PCBN material according to claim 25, which does not include abrasive media impurity.

27. the PCBN material according to claim 25 or 26, wherein abrasive media impurity includes selected from tungsten carbide, carbonization Any material in silicon, aluminium oxide, zirconium oxide, titanium carbide and boron carbide.

28. according to claim 25,26 or 27 described in any item PCBN materials, wherein the cBN particle has 0.2 to 15 μm Average-size.

29. according to the described in any item PCBN materials of claim 25-28, wherein the cBN particle has being averaged greater than 1 μm Size.

30. according to the described in any item PCBN materials of claim 25-29, wherein the cBN particle has multi-modal be averaged Size distribution.

31. according to the described in any item PCBN materials of claim 25-30, wherein the PCBN material includes less than 80 volume % CBN particle.

32. according to the described in any item PCBN materials of claim 25-31, wherein the host material includes in titanium and aluminium The material of any compound.

33. PCBN material according to claim 32, wherein the host material includes titanium carbonitride, titanium carbide, nitridation It is any in titanium, titanium diboride, aluminium nitride and aluminium oxide.

34. a kind of tool, it includes according to the described in any item sintered polycrystalline materials of claim 25-33, the tool is for cutting Cut, milling, grind, drilling or it is other grinding application in it is any.